CN110157331A - A kind of corrosion-resistant epoxy paint and preparation method thereof - Google Patents
A kind of corrosion-resistant epoxy paint and preparation method thereof Download PDFInfo
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- CN110157331A CN110157331A CN201910464246.7A CN201910464246A CN110157331A CN 110157331 A CN110157331 A CN 110157331A CN 201910464246 A CN201910464246 A CN 201910464246A CN 110157331 A CN110157331 A CN 110157331A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/10—Block or graft copolymers containing polysiloxane sequences
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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Abstract
The invention discloses a kind of corrosion-resistant epoxy paint and preparation method thereof, which includes the raw material of following parts by weight: 100 parts of modified epoxy, 80-120 parts of pigments and fillers, 2-5 parts of dispersing agent, 15-20 parts of coalescing agent, 1-3 parts of levelling agent, 1-3 parts of defoaming agent；Under the premise of not influencing epoxy resin viscosity, by the way of being modified to epoxy resin, active anti-corrosion functional group is introduced into epoxy resin by the method being grafted, so that epoxy coating has good scrub resistance, its corrosion-resistant function mechanism is not easily to fall off, the corrosion resistance of maintenance epoxy coating that can be permanent.
Description
Technical field
The invention belongs to technical field of coatings, and in particular to a kind of corrosion-resistant epoxy paint and preparation method thereof.
Background technique
Epoxy resin is a kind of important thermosetting resin, and the epoxy resin after solidification has good electric property, glues
The advantages that connecing performance and mechanical property, is widely used in the fields such as machining, aerospace, a large amount of in epoxy molecule chain
Rigid phenyl ring imparts resin rigidity and heat resistance；Hydroxyl and ehter bond isopolarity group, then it is right after epoxy resin cure to make
Base metal has stronger adhesion property, but the corrosion resistance of epoxy resin itself and high temperature resistance are poor, existing skill
It in art, often adds some modifying agent and it is modified, but the durability of the epoxy resin of physical modification is poor, chemical modification
Frequently with the method with the epoxy terminated grafting of epoxy resin, the method can reduce the adhesion property of epoxy resin, cause modified
Epoxy resin adhesiveness die down, the epoxy coating after coating is easy to fall off.
Summary of the invention
The purpose of the present invention is to provide a kind of corrosion-resistant epoxy paints and preparation method thereof, are not influencing epoxy resin viscosity
Under the premise of, by the way of being modified to epoxy resin, active anti-corrosion functional group is introduced by the method being grafted
In epoxy resin, so that epoxy coating has good scrub resistance, corrosion-resistant function mechanism is not easily to fall off, can be permanent
Maintenance epoxy coating corrosion resistance.
The technical problem to be solved in the invention are as follows:
1, how under the premise of not changing epoxy resin adhesion property, raising corrosion resistance is modified to it；
2, organosilicon is added in epoxy resin by the prior art with independent additive, due to the low superficiality of organosilicon
Can, keep it poor with the compatibility and compatibility of epoxy resin or coating other components；
3, how the corrosion resistance of permanent maintenance epoxy resin.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of corrosion-resistant epoxy paint, the raw material including following parts by weight: 100 parts of modified epoxy, pigments and fillers 80-120
Part, 2-5 parts of dispersing agent, 15-20 parts of coalescing agent, 1-3 parts of levelling agent, 1-3 parts of defoaming agent；
The modified epoxy the preparation method comprises the following steps:
S1,1mol3- propenyl and catalyst are added in reaction flask, are passed through nitrogen protection, are warming up to 50-55 DEG C, delayed
Slowly 1.1-1.2mol epoxychloropropane is added dropwise, is added dropwise in 1h, then continue to be stirred to react 2h, after reaction,
Vacuum distillation removes unreacted epoxychloropropane, in addition to this, arrives compound A crude product, reaction equation without other processing
It is as follows:
200ml tert-pentyl alcohol is added in S2, the compound A crude product prepared to S1, is subsequently added into 1mol octadecylamine, is heated to
115-120 DEG C, stirring carries out substitution reaction 4-5h, after reaction, is cooled to 70-80 DEG C, and 100ml mass fraction is added and is
30% sodium hydrate aqueous solution continues to stir 1h, and after reaction, purified to get compound B is arrived, reaction equation is as follows:
S3, the compound B that step S2 is obtained is dissolved in 200ml toluene, 5mmol cesium carbonate is added, after mixing evenly, led to
Enter nitrogen protection, be warming up to 50-55 DEG C, is slowly added dropwise 2.1-2.3mol epoxychloropropane, is added dropwise in 2h, then
Continue to be stirred to react 3-4h, obtains the crude liquid of compound C；
S4, the crude liquid of step S3 compound C is warming up to 45-50 DEG C, the hydrogen that 300ml mass fraction is 30% is added dropwise
Sodium hydroxide solution is added dropwise in 1h, then continues to be stirred to react 1h, and after reaction, 200ml is added into filtrate for filtering
Ethyl acetate, liquid separation remove water layer, and 200ml deionized water then is added to ethyl acetate layer and is washed, remaining hydrogen is removed
Sodium oxide molybdena and sodium chloride, liquid separation, ethyl acetate layer remove solvent and extra epoxychloropropane through rotary evaporation to get chemical combination is arrived
Object D；
S5, compound D, platinum catalyst and 500ml toluene prepared by step S4 are added in back flow reaction device, are heated
It is warming up to 55-60 DEG C, 1mol containing hydrogen silicone oil is added dropwise dropwise, is added dropwise in 1h, then continues to be warming up to 110-120 DEG C, reflux
6-8h is reacted, it is after reaction, purified to obtain modifying agent E；
The reaction process of S3-S5 is as follows:
The preparation of S6 modified epoxy
1kg epoxy resin is added in reaction kettle, 150-200g modifying agent E is subsequently added into and is warming up to after mixing evenly
95-100 DEG C, 20-30ml triethylamine is then added dropwise, is added dropwise in 30min, heat preservation continues to be stirred to react 2-3h, i.e.,
Obtain modified epoxy.
Further, catalyst described in step S1 is tin tetrachloride, and the additional amount of catalyst is 2mmol.
Further, purifying described in step S2 specifically: after reaction, be cooled to room temperature, filter, be added into filtrate
200ml ethyl acetate, liquid separation remove water layer, and 200ml deionized water then is added to ethyl acetate layer and is washed, removes residual
The sodium hydroxide and sodium chloride stayed, liquid separation, ethyl acetate layer remove solvent through rotary evaporation to get compound B is arrived.
Further, platinum catalyst described in step S5 is Pt (PPh3)4, the additional amount of catalyst is 5mmol.
Further, purifying described in step S5 specifically: after reaction, be cooled to room temperature, vacuum fractionation removes small point
1g active carbon and 200ml ether is added in sub- compound, and being heated to back flow reaction 2-3h to reaction solution is colourless rear stopping, being centrifuged
Separation, obtained centrifugal liquid arrive modifying agent E after vacuum distillation removes solvent.
A kind of preparation method of corrosion-resistant epoxy paint, specifically: by corrosion-resistant epoxy paint each raw material investment compounding jar into
Row premix 5-10min, then carries out melting extrusion, the extrusion parameter for pre-composition are as follows: 120 DEG C of an area, two 180 DEG C of areas,
Screw speed 50Hz extruding sheet object, which is put into ball mill, to be ground, and the revolving speed of ball mill is 1600-2200rpm, grinding
Coarse powder crosses 200 meshes by rotation sub-sieve and obtains 10-80 microns of fine powder as final corrosion-resistant epoxy paint.
Beneficial effects of the present invention:
The present invention provides a kind of corrosion-resistant epoxy paints, under the premise of not influencing epoxy resin viscosity, using to epoxy
Active anti-corrosion functional group is introduced into epoxy resin by the mode that resin is modified by the method being grafted, specifically: it is first
First 3- propenyl has obtained compound A under the action of catalyst tin tetrachloride, with epoxychloropropane ring-opening reaction, then to change
It closes and octadecylamine is added in object A crude product, compound A and octadecylamine occur nucleophilic substitution and obtained compound B, then compound
B under alkaline condition with excessive epichlorohydrin reaction, wherein the epoxychloropropane of a molecule and the hydroxyl on compound B are anti-
It answers, the epoxychloropropane and the imine reaction on compound B of another molecule, to obtain compound C, compound C is in hydrogen-oxygen
Under the action of changing sodium water solution, obtained containing there are two the compound D of epoxy group, compound D under the action of Pt catalyst with
Hydrosilylation occurs for containing hydrogen silicone oil, to obtain modifying agent E, finally, the work of modifying agent E and epoxy resin in triethylamine
Under, ring-opening reaction occurs for the epoxy group on the alcoholic extract hydroxyl group and modifying agent on epoxy resin, so that modifying agent E grafting is embedded into
In epoxy resin, epoxy terminated due to epoxy resin is not engaged in reaction, so and having not been changed the original viscosity of epoxy resin；
Modifying agent E is grafted on epoxy resin in a manner of chemical bond, i.e., hydrophobic aliphatic long-chain octadecyl and will be had
Machine silicone grease is firmly introduced into epoxy resin in a manner of being bonded, the introducing of fatty long-chain increase epoxy resin water resistance and
The self-cleaning of epoxy coating can be improved in corrosion resistance；It is special resistance to that the Si-O key contained in organosilicon has it
The bond energy of hot and flexibility, silicon oxygen bond is higher than carbon-carbon bond, the thermal stability of epoxy resin is increased, to widen asphalt mixtures modified by epoxy resin
The application range of rouge further imparts the certain hydrophobic performance of epoxy resin since organosilicon has lower surface energy
And corrosion resistance, the organosilicon that epoxy resin is introduced into a manner of bonding is more stable, it is not susceptible to phenomenon of phase separation, thus
It solves the prior art and is added to organosilicon in epoxy resin with independent additive, due to the low surface property of organosilicon,
The problem for keeping it poor with the compatibility and compatibility of epoxy resin or coating other components；
It is firmly introduced into a manner of being bonded just because of corrosion resistant hydrophobic fat long-chain octadecyl and organic silicone grease
In epoxy resin, so that epoxy coating has good scrub resistance, corrosion-resistant function mechanism is not easily to fall off, can be permanent
Maintenance epoxy coating corrosion resistance.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's all other embodiment obtained without creative efforts belongs to the model that the present invention protects
It encloses.
In following embodiments, modified epoxy the preparation method comprises the following steps:
S1,1mol3- propenyl and 2mmol catalyst tin tetrachloride are added in reaction flask, are passed through nitrogen protection, risen
Temperature is slowly added dropwise 1.2mol epoxychloropropane, is added dropwise in 1h to 55 DEG C, then continues to be stirred to react 2h, reaction
After, vacuum distillation removes unreacted epoxychloropropane, in addition to this, without other processing to get thick to compound A
Product, reaction equation are as follows:
The mass spectral results of gained compound A are as follows: HRMS m/z (ESI+)calcd for C6H11ClO2([M+1]+),
151.0524；
200ml tert-pentyl alcohol is added in S2, the compound A crude product prepared to S1, is subsequently added into 1mol octadecylamine, is heated to
120 DEG C, stirring carries out substitution reaction 5h and is cooled to 70 DEG C after reaction, and the sodium hydrate aqueous solution of 100ml30% is added,
Continue to stir 1h, be cooled to room temperature, filter, 200ml ethyl acetate is added into filtrate, liquid separation removes water layer, then to acetic acid
Methacrylate layer is added 200ml deionized water and is washed, and removes remaining sodium hydroxide and sodium chloride, liquid separation, ethyl acetate layer warp
Rotary evaporation removes solvent to get compound B is arrived, and reaction equation is as follows:
The mass spectral results of gained compound B are as follows: HRMS m/z (ESI+)calcd for C24H49NO2([M+1]+),
384.3538；
S3, the compound B that step S2 is obtained is dissolved in 200ml toluene, 5mmol cesium carbonate is added, after mixing evenly, led to
Enter nitrogen protection, be warming up to 55 DEG C, be slowly added dropwise 2.2mol epoxychloropropane, be added dropwise in 2h, then continues to stir
Reaction 3h is mixed, the crude liquid of compound C is obtained；
The mass spectral results of gained compound C are as follows: HRMS m/z (ESI+)calcd for C30H58ClNO4([M+1]+),
532.1465；
S4, the crude liquid of step S3 compound C is warming up to 45 DEG C, the hydrogen-oxygen that 300ml mass fraction is 30% is added dropwise
Change sodium solution, be added dropwise in 1h, then continue to be stirred to react 1h, after reaction, 200ml second is added into filtrate for filtering
Acetoacetic ester, liquid separation remove water layer, and 200ml deionized water then is added to ethyl acetate layer and is washed, remaining hydrogen-oxygen is removed
Change sodium and sodium chloride, liquid separation, ethyl acetate layer removes solvent and extra epoxychloropropane through rotary evaporation to get compound is arrived
D；
The mass spectral results of gained compound D are as follows: HRMS m/z (ESI+)calcd for C30H57NO4([M+1]+),
496.1241；
S5, the compound D, 5mmol catalyst Pt (PPh for preparing step S43)4Back flow reaction is added to 500ml toluene
In device, 60 DEG C are heated to, 1mol containing hydrogen silicone oil is added dropwise dropwise, is added dropwise in 1h, then continues to be warming up to 110 DEG C,
Back flow reaction 7h is cooled to room temperature after reaction, and vacuum fractionation removes small molecule compound, and 1g active carbon and 200ml is added
Ether, being heated to back flow reaction 2h to reaction solution is colourless rear stopping, being centrifugated, obtained centrifugal liquid is removed through vacuum distillation
It goes after solvent to get to modifying agent E；
The reaction process of S3-S5 is as follows:
The IR Characterization of modifying agent E is as follows: IR (KBr):2922(-CH2-、-CH3), 1659 (- C=
O-),1376(-CH3), 1293,1205 (- C-N), 1180 (- O-Si-C-), 914 (epoxy group) cm-1。
The preparation of S6 modified epoxy
1kg epoxy resin is added in reaction kettle, 200g modifying agent E is subsequently added into and is warming up to 100 after mixing evenly
DEG C, 25ml triethylamine is then added dropwise, is added dropwise in 30min, heat preservation continues to be stirred to react 2h to get modified epoxy is arrived
Resin；
The structure of possible modified epoxy is as follows:
Alcoholic extract hydroxyl group on epoxy resin can be reacted with two epoxy groups on modifying agent E or a molecule changes
Property agent E and 2 molecules cross linking of epoxy resin, thus by modifying agent E insertion be grafted in epoxy resin；
The IR Characterization of modified epoxy is as follows: IR (KBr):3032,3005 (benzene
Ring), 2964,2920 (- CH2-、-CH3),1375(-CH3), 1294,1205 (- C-N), 1180 (- O-Si-C-), 915 (epoxies
Base) cm-1。
Embodiment 1
A kind of corrosion-resistant epoxy paint, the raw material including following weight: modified epoxy 100g, pigments and fillers 80g, dispersing agent
5g, coalescing agent 15g, levelling agent 1g, defoaming agent 1g；
A kind of corrosion-resistant epoxy paint premixes the preparation method comprises the following steps: each raw material of corrosion-resistant epoxy paint is put into compounding jar
Pre-composition is then carried out melting extrusion, the extrusion parameter by 5min are as follows: 120 DEG C of an area, two 180 DEG C of areas, screw speed
50Hz extruding sheet object, which is put into ball mill, to be ground, and the revolving speed of ball mill is 2200rpm, and the coarse powder of grinding passes through rotation sub-sieve
It crosses 200 meshes and obtains 10-80 microns of fine powder as final corrosion-resistant epoxy paint.
Embodiment 2
A kind of corrosion-resistant epoxy paint, the raw material including following weight: modified epoxy 100g, pigments and fillers 120g, dispersion
Agent 2g, coalescing agent 20g, levelling agent 3g, defoaming agent 3g；
A kind of corrosion-resistant epoxy paint premixes the preparation method comprises the following steps: each raw material of corrosion-resistant epoxy paint is put into compounding jar
Pre-composition is then carried out melting extrusion, the extrusion parameter by 10min are as follows: 120 DEG C of an area, two 180 DEG C of areas, screw speed
50Hz extruding sheet object, which is put into ball mill, to be ground, and the revolving speed of ball mill is 1600rpm, and the coarse powder of grinding passes through rotation sub-sieve
It crosses 200 meshes and obtains 10-80 microns of fine powder as final corrosion-resistant epoxy paint.
Embodiment 3
A kind of corrosion-resistant epoxy paint, the raw material including following weight: modified epoxy 100g, pigments and fillers 100g, dispersion
Agent 4g, coalescing agent 18g, levelling agent 2g, defoaming agent 2g；
A kind of corrosion-resistant epoxy paint premixes the preparation method comprises the following steps: each raw material of corrosion-resistant epoxy paint is put into compounding jar
Pre-composition is then carried out melting extrusion, the extrusion parameter by 8min are as follows: 120 DEG C of an area, two 180 DEG C of areas, screw speed
50Hz extruding sheet object, which is put into ball mill, to be ground, and the revolving speed of ball mill is 2000rpm, and the coarse powder of grinding passes through rotation sub-sieve
It crosses 200 meshes and obtains 10-80 microns of fine powder as final corrosion-resistant epoxy paint.
Comparative example 1
A kind of corrosion-resistant epoxy paint, the raw material including following weight: epoxy resin 100g, pigments and fillers 100g, dispersing agent 4g,
Coalescing agent 18g, levelling agent 2g, defoaming agent 2g；
The preparation method of corrosion-resistant epoxy paint is the same as embodiment 3.
Comparative example 2
A kind of corrosion-resistant epoxy paint, the raw material including following weight: epoxy resin 95g, containing hydrogen silicone oil 5g, pigments and fillers
100g, dispersing agent 4g, coalescing agent 18g, levelling agent 2g, defoaming agent 2g；
The preparation method of corrosion-resistant epoxy paint is the same as embodiment 3.
The performance test of corrosion-resistant epoxy paint is as follows:
(1) contact angle test
The embodiment 1-3 and comparative example 1-2 coating prepared is coated at coating on steel plate, and it is contacted respectively
Angle test, test result are as shown in Table 1:
The contact angle of table one, epoxy anticorrosive coating
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | |
| Contact angle/° | 122.3 | 124.8 | 125.7 | 76.5 | 88.1 |
As shown in Table 1, in coating film forming procedure, segment containing Si and hydrophobic aliphatic long-chain octadecyl are easier to migrate out
The surface of coating, since the slipping and hydrophobicity of Si and the strong-hydrophobicity of fatty long-chain octadecyl make film and water
Contact angle becomes larger, and considerably increases the water resistance of corrosion-resistant epoxy paint.
(2) corrosion-resistant test
The embodiment 1-3 and comparative example 1-2 coating prepared is coated on steel plate into coating, matter is respectively adopted in corrosion resistance
The hydrochloric acid solution for measuring sodium hydroxide solution and 20wt% that score is 40wt% impregnates coated steel plates, and recording surface occurs obvious broken
The time split, specific test result see the table below two:
The corrosion-resistant test of table two, Synthetic Leather
As shown in Table 3, corrosion-resistant epoxy paint of the present invention has good corrosion resistance.
The above content is just an example and description of the concept of the present invention, affiliated those skilled in the art
It makes various modifications or additions to the described embodiments or is substituted in a similar manner, without departing from invention
Design or beyond the scope defined by this claim, be within the scope of protection of the invention.
Claims (6)
1. a kind of corrosion-resistant epoxy paint, it is characterised in that: the raw material including following parts by weight: 100 parts of modified epoxy, face are filled out
Expect 80-120 parts, 2-5 parts of dispersing agent, 15-20 parts of coalescing agent, 1-3 parts of levelling agent, 1-3 parts of defoaming agent；
The modified epoxy the preparation method comprises the following steps:
S1,1mol3- propenyl and catalyst are added in reaction flask, are passed through nitrogen protection, be warming up to 50-55 DEG C, slowly by
It is added dropwise to 1.1-1.2mol epoxychloropropane, is added dropwise in 1h, then continues to be stirred to react 2h, after reaction, decompression
Unreacted epoxychloropropane is distilled off, in addition to this, arrives compound A crude product without other processing, reaction equation is such as
Under:
200ml tert-pentyl alcohol is added in S2, the compound A crude product prepared to S1, is subsequently added into 1mol octadecylamine, is heated to 115-
120 DEG C, stirring carries out substitution reaction 4-5h, after reaction, is cooled to 70-80 DEG C, and it is 30% that 100ml mass fraction, which is added,
Sodium hydrate aqueous solution continues to stir 1h, and after reaction, purified to get compound B is arrived, reaction equation is as follows:
S3, the compound B that step S2 is obtained is dissolved in 200ml toluene, 5mmol cesium carbonate is added and is passed through nitrogen after mixing evenly
Gas shielded is warming up to 50-55 DEG C, is slowly added dropwise 2.1-2.3mol epoxychloropropane, is added dropwise in 2h, then continues to
It is stirred to react 3-4h, obtains the crude liquid of compound C；
S4, the crude liquid of step S3 compound C is warming up to 45-50 DEG C, the hydroxide that 300ml mass fraction is 30% is added dropwise
Sodium solution is added dropwise in 1h, then continues to be stirred to react 1h, and after reaction, 200ml acetic acid is added into filtrate for filtering
Ethyl ester, liquid separation remove water layer, and 200ml deionized water then is added to ethyl acetate layer and is washed, remaining hydroxide is removed
Sodium and sodium chloride, liquid separation, ethyl acetate layer remove solvent and extra epoxychloropropane through rotary evaporation to get compound D is arrived；
S5, compound D, platinum catalyst and 500ml toluene prepared by step S4 are added in back flow reaction device, heat temperature raising
To 55-60 DEG C, 1mol containing hydrogen silicone oil is added dropwise dropwise, is added dropwise in 1h, then continues to be warming up to 110-120 DEG C, back flow reaction
6-8h, it is after reaction, purified to obtain modifying agent E；
The reaction process of S3-S5 is as follows:
The preparation of S6 modified epoxy
1kg epoxy resin is added in reaction kettle, 150-200g modifying agent E is subsequently added into and is warming up to 95- after mixing evenly
100 DEG C, 20-30ml triethylamine is then added dropwise, is added dropwise in 30min, heat preservation continues to be stirred to react 2-3h to get arriving
Modified epoxy.
2. a kind of corrosion-resistant epoxy paint according to claim 1, it is characterised in that: catalyst described in step S1 is tetrachloro
Change tin, the additional amount of catalyst is 2mmol.
3. a kind of corrosion-resistant epoxy paint according to claim 1, it is characterised in that: purifying described in step S2 specifically:
After reaction, it is cooled to room temperature, is filtered, 200ml ethyl acetate is added into filtrate, liquid separation removes water layer, then to acetic acid
Methacrylate layer is added 200ml deionized water and is washed, and removes remaining sodium hydroxide and sodium chloride, liquid separation, ethyl acetate layer warp
Rotary evaporation removes solvent to get compound B is arrived.
4. a kind of corrosion-resistant epoxy paint according to claim 1, it is characterised in that: platinum catalyst described in step S5 is Pt
(PPh3)4, the additional amount of catalyst is 5mmol.
5. a kind of corrosion-resistant epoxy paint according to claim 1, it is characterised in that: purifying described in step S5 specifically:
After reaction, it is cooled to room temperature, vacuum fractionation removes small molecule compound, and 1g active carbon and 200ml ether is added, is heated to
Back flow reaction 2-3h is colourless rear stopping to reaction solution, is centrifugated, after obtained centrifugal liquid is evaporated under reduced pressure removing solvent,
Obtain modifying agent E.
6. a kind of preparation method of corrosion-resistant epoxy paint as described in claim 1, it is characterised in that: specifically: epoxy is prevented
Premix 5-10min is carried out in rotten each raw material investment compounding jar of coating, pre-composition is then subjected to melting extrusion, the extrusion ginseng
Number are as follows: 120 DEG C of an area, two 180 DEG C of areas, screw speed 50Hz extruding sheet object, which is put into ball mill, to be ground, ball mill
Revolving speed is 1600-2200rpm, and the coarse powder of grinding crosses 200 meshes by rotation sub-sieve and obtains 10-80 microns of fine powder as final ring
Oxygen anticorrosive paint.
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| CN201910464246.7A CN110157331B (en) | 2019-05-30 | 2019-05-30 | Epoxy anticorrosive paint and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110982078A (en) * | 2019-11-25 | 2020-04-10 | 江南大学 | Polysiloxane-containing multi-block polymer, composition prepared from same and preparation method of composition |
| CN113307984A (en) * | 2021-04-29 | 2021-08-27 | 广西桂林荣鑫新材料科技有限公司 | Preparation method of aqueous epoxy resin dispersion |
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| CN102863876A (en) * | 2012-09-06 | 2013-01-09 | 中科院广州化学有限公司 | Organic silicon modified epoxy floor paint and preparation method and application thereof |
| CN107083133A (en) * | 2017-06-17 | 2017-08-22 | 合肥市晨雷思建筑材料科技有限公司 | A kind of anticorrosive paint and preparation method thereof |
| CN107880720A (en) * | 2017-11-24 | 2018-04-06 | 靖江市新东机械零部件制造有限公司 | A kind of steel pipe corrosion-proof composite coating and preparation method thereof |
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2019
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102863876A (en) * | 2012-09-06 | 2013-01-09 | 中科院广州化学有限公司 | Organic silicon modified epoxy floor paint and preparation method and application thereof |
| CN107083133A (en) * | 2017-06-17 | 2017-08-22 | 合肥市晨雷思建筑材料科技有限公司 | A kind of anticorrosive paint and preparation method thereof |
| CN107880720A (en) * | 2017-11-24 | 2018-04-06 | 靖江市新东机械零部件制造有限公司 | A kind of steel pipe corrosion-proof composite coating and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110982078A (en) * | 2019-11-25 | 2020-04-10 | 江南大学 | Polysiloxane-containing multi-block polymer, composition prepared from same and preparation method of composition |
| CN113307984A (en) * | 2021-04-29 | 2021-08-27 | 广西桂林荣鑫新材料科技有限公司 | Preparation method of aqueous epoxy resin dispersion |
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